15β-substituted estrone derivatives as selective inhibitors of 17β-hydroxysteroid-dehydrogenases, method of preparation and use thereof
a technology of hydroxysteroid dehydrogenases and estrone derivatives, which is applied in the field of 15substituted estrone derivatives as selective inhibitors of 17hydroxysteroid dehydrogenases, method of preparation and use thereof, can solve the problems of recurrence, resistance, and large effort still dedicated to searching, and achieve the effect of not cytotoxi
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example 1
ldimethylsilyloxy)-estra-1,3,5(10),15-tetraen-17-one (1)
[0147]
[0148]Enone 1 was prepared according to a published method (Sakakibara, M.; Uchida, A. O. Biosci. Biotech. Biochchem 1996, 60, 3, 405) by Saegusa oxidation in 75% yield: mp 148° C.; [α]D −37.4 (c 0.203; CHCl3); 1H NMR (500 MHz, CDCl3) δ 0.19 (s, 6H, Si—(CH3)2), 0.98 (s, 9H, (CH3)3—C), 1.11 (s, 3H, H-18), 1.55 (m, 1H, H-7a), 1.66-1.85 (m, 3H, H-8, 11a, 12a), 2.01 (m, 1H, H-12b), 2.18 (dm, 1H, J=12.9 Hz, H-7b), 2.33 (m, 1H, H-9), 2.43 (m, 1H, H-11a), 2.50 (dm, 1H, J=11.6 Hz, H-14), 2.87-2.96 (m, 2H, H-6), 6.08 (dd, 1H, J=6.0; 3.2 Hz, H-16), 6.59 (bd, 1H, J=2.7 Hz, H-4), 6.64 (dd, 1H, J=8.5; 2.7 Hz, H-2), 7.12 (d, 1H, J=8.5 Hz, H-8), 7.63 (dd, 1H, J=6.0; 1.9 Hz, H-15); 13C NMR (150.9 MHz, CDCl3) δ−4.41 (Si—(CH3)2), 181.5 (C—(CH3)3), 20.97 (C-18), 25.34 (C-11), 25.67 (C—(CH3)3), 26.68 (C-7), 29.08 and 29.19 (C-6, 12), 35.48 (C-8), 45.15 (C-9), 51.46 (C-13), 56.13 (C-14), 117.33 (C-3), 120.01 (C-4), 125.82 (C-1), 131.87 (C-16)...
example 2
ldimethylsilyloxy)-15β-vinyl-estra-1,3,5(10)-trien-17-one (2)
[0149]
[0150]To our knowledge, the preparation of 15β-vinylestrone was published only in WO200834796. We altered this method so that instead of the benzyl protecting group (giving a reaction yield of 24%) a t-butyldimethylsilyl group was now used. We succeeded to significantly increase yields of vinylestrone 2, which (after crystallization from EtOAc) are reproducibly above 90%.
[0151]Mixture of 1 mol·l−1 solution of vinylmagnesium bromide in THF (13 ml, 13.08 mmol), CuI (65 mg, 0.654 mmol) and HMPA (2.8 ml, 15.7 mmol) in CH2Cl2 (50 ml) under argon atmosphere was cooled to −78° C. A solution of enone 1 (2.5 g, 6.54 mmol) and TMSCl (1.7 ml, 13.08 mmol) in CH2Cl2 (50 ml) was added dropwise to this mixture. The reaction mixture was then slowly warmed to room temperature and stirred overnight. After adding water and dropwise addition of 1 mol·l−1 HCl, the mixture was stirred for 5 minutes, then diluted with CH2Cl2 and washed wit...
example 3
thyl-3-hydroxy-estra-1,3,5(10)-trien-17-one (3)
[0155]
[0156]Compound 3 was prepared according to the above general procedure by reacting vinylestrone 2 with styrene (56 μl). Chromatography on HPLC (30 / 70 MeCN / H2O, tR=15 min) yielded 36 mg of colorless solid 3 (numbering of the C-15 side chain in all the following examples is the same as in derivative 3): mp 153° C.; [α]D+52.6 (c 0.547; CHCl3); 1H NMR (500 MHz, CDCl3) δ 1.03 (s, 3H, H-18), 1.35-1.55 (m, 3H, H-7a, 11a, 12a), 1.62-1.76 (m, 3H, H-8, 14, 1′a), 1.86-1.97 (m, 3H, H-7a, 12b, 1′b), 2.25 (m, 1H, H-9), 2.30-2.38 (m, 2H, H-11b, 15), 2.40 (dd, 1H, J=19.3; 2.8 Hz, H-16a), 2.49 (dd, 1H, J=19.3; 8.1 Hz, H-16b), 2.54 (ddd, 1H, J=13.6; 9.2; 7.1 Hz, H-2′a), 2.75 (ddd, 1H, J=13.6; 9.8; 5.2 Hz, H-2′b), 2.80-2.93 (m, 2H, H-6), 4.82 (bs, 1H, OH), 6.59 (dm, 1H, J=2.8 Hz, H-4), 6.63 (ddm, 1H, J=8.4; 2.8 Hz, H-2), 7.13 (dd, 1H, J=8.5; 1.1 Hz, H-1), 7.18 (m, 2H, H-2″), 7.21 (m, 1H, H-4″), 7.30 (m, 2H, H-3″); 13C NMR (150.9 MHz, CDCl3) δ 17.71 ...
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